HRID1756007

反应详情

EQUATION

反应方程式

HRID 1756007 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

p-Toluenesulfonic acid (0.10 g) was added to a solution of ethyl 4-(2-(4-(2-(tetrahydropyran-2-yloxy)ethyl)phenyl)ethylamino)-6-ethylpyrimidine-5-carboxylate (4.20 g, 9.82 mmol) in ethanol (40 ml). The mixture was heated under reflux for 4 hours. After cooling to room temperature, the solvent was evaporated under reduced pressure. Water (40 ml) was added to the residue. The mixture was extracted with methylene chloride and dried over magnesium sulfate. After evaporation of the solvent, the residue was purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (=1/1) to give the desired ethyl 4-(2-(4-(2-hydroxyethyl)phenyl)ethylamino)-6-ethylpyrimidine-5-carboxylate (2.60 g, 77%).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 4 hours
  3. customthe solvent was evaporated under reduced pressure
  4. additionWater (40 ml) was added to the residue
  5. extractionThe mixture was extracted with methylene chloride
  6. dry with materialdried over magnesium sulfate
  7. customAfter evaporation of the solvent
  8. customthe residue was purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (=1/1)